CN115317942A - Parallel type solid-containing mother liquor solvent continuous rectification recovery system and method and application thereof - Google Patents
Parallel type solid-containing mother liquor solvent continuous rectification recovery system and method and application thereof Download PDFInfo
- Publication number
- CN115317942A CN115317942A CN202211040643.XA CN202211040643A CN115317942A CN 115317942 A CN115317942 A CN 115317942A CN 202211040643 A CN202211040643 A CN 202211040643A CN 115317942 A CN115317942 A CN 115317942A
- Authority
- CN
- China
- Prior art keywords
- distillation
- kettle
- solvent
- mother liquor
- solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002904 solvent Substances 0.000 title claims abstract description 117
- 239000007787 solid Substances 0.000 title claims abstract description 82
- 239000012452 mother liquor Substances 0.000 title claims abstract description 63
- 238000011084 recovery Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000004821 distillation Methods 0.000 claims abstract description 282
- 238000007599 discharging Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000011343 solid material Substances 0.000 claims description 5
- 101100134058 Caenorhabditis elegans nth-1 gene Proteins 0.000 claims description 4
- FAPWYRCQGJNNSJ-UBKPKTQASA-L calcium D-pantothenic acid Chemical compound [Ca+2].OCC(C)(C)[C@@H](O)C(=O)NCCC([O-])=O.OCC(C)(C)[C@@H](O)C(=O)NCCC([O-])=O FAPWYRCQGJNNSJ-UBKPKTQASA-L 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims 1
- 238000005194 fractionation Methods 0.000 abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 27
- 239000012071 phase Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- 239000007789 gas Substances 0.000 description 13
- 238000001704 evaporation Methods 0.000 description 11
- 230000008020 evaporation Effects 0.000 description 11
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000001944 continuous distillation Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
Abstract
The invention discloses a parallel type continuous solvent rectification and recovery system containing solid mother liquor and a method thereof, wherein the parallel type continuous solvent rectification and recovery system containing the solid mother liquor comprises a distillation assembly, a discharge pump, a rectification tower, a reboiler and a tower top condenser, the distillation assembly comprises a plurality of distillation kettles, the plurality of distillation kettles are connected in parallel, the bottoms of the plurality of distillation kettles of the discharge pump are independently or jointly connected with a discharge pipe for discharging, the top of each distillation kettle is connected with the rectification tower through a pipeline, the top of each distillation kettle is connected with the pipeline of the rectification tower and is respectively provided with a control valve, the rectification tower is used for collecting steam of the distillation assembly and conducting fractionation to form light fraction and heavy fraction, the reboiler is connected with the bottom of the rectification tower, and the tower top condenser is connected with the top of the rectification tower. The parallel continuous solvent rectification and recovery system for the solid-containing mother liquor can achieve the purposes of saving equipment, saving energy, keeping the intake components basically constant and ensuring the rectification quality.
Description
Technical Field
The invention relates to the technical field of medicine and chemical industry, in particular to a parallel type solid-containing mother liquor solvent continuous rectification recovery system and a method and application thereof.
Background
The solvent containing the solid mother liquor is required to be recovered in pharmaceutical factories and chemical factories, and the solvent containing the solid mother liquor has the general property that the solid is usually dissolved in the solvent. The solid in the initial state of the mother liquor is not separated out, the content of the solvent is gradually reduced along with the rectification, the solid originally dissolved in the liquid is completely separated out, and at the moment, if the continuous rectification is carried out, the separated solid can be accumulated on a tower plate of a rectification tower or in a gas-liquid channel of a regular packing, so that the tower body of the rectification tower is blocked. Therefore, the traditional treatment method for recovering the solvent containing the solid mother liquor has two kinds, one is to evaporate the solvent from the mother liquor by a simple evaporation mode, then to collect the condensate containing the solvent and not containing the solid and the mother liquor containing the solid and not containing the solvent respectively, and then to treat the solvent and the solid respectively. Another method is batch rectification, which leaves the solid in a kettle while rectifying, and the method needs more towers and kettles, often more than ten. The two traditional treatment methods have the advantages and the disadvantages respectively, and have the common disadvantages of high energy consumption, high equipment investment, multiple evaporation and condensation processes, high consumption of steam and circulating cooling water and high energy consumption of the whole product.
Disclosure of Invention
Based on this, the solvent continuous rectification recovery system of the parallel solid-containing mother liquor is provided, aiming at the problems that the traditional treatment method has large energy consumption, large equipment investment, multiple evaporation and condensation processes and large consumption of steam and circulating cooling water. The parallel type continuous solvent rectification and recovery system for the solid-containing mother liquor saves energy by directly utilizing the enthalpy of steam, combines a plurality of independent intermittent rectification towers into one continuous rectification tower, changes the original independent intermittent rectification kettles into distillation kettles, and is arranged in a linkage manner, so that the proportion of steam components entering the rectification tower in the whole process is basically constant, and thus, all the setting and adjustment parameters of the rectification tower can be basically fixed, equipment is saved, and the rectification quality is improved.
The utility model provides a solvent continuous rectification recovery system of solid mother liquor is contained to parallel, includes distillation subassembly, rectifying column, reboiler and overhead condenser, the distillation subassembly includes a plurality of stills, and is a plurality of stills parallel connection, it is a plurality of the discharging pipe is connected alone or jointly at the bottom of stills's the cauldron in order to be used for the ejection of compact, each stills's top all connect in through the pipeline the rectifying column, each stills's top connect in be provided with control flap on the pipeline of rectifying column respectively, the rectifying column is used for collecting the steam of distillation subassembly and fractionate and form light fraction and heavy fraction, the reboiler connect in the bottom of rectifying column is in order to be used for reboiling to heavy fraction, overhead condenser connect in the top of rectifying column is in order to be used for the rectifying column light fraction to condense.
In some embodiments, the solvent continuous rectification recovery system for the parallel solid-containing mother liquor further comprises a discharge pump and a product storage tank, wherein the discharge pump is connected with the discharge pipe, and the product storage tank is connected with the discharge pump for collecting the concentrated solid-containing liquid at the bottom of the distillation still.
In some of these embodiments, the number of stills is 5 to 8.
In some of these embodiments, the still pot has a volume of 2m 3 ～12m 3 。
In some of the embodiments, a liquid level meter is arranged in each distillation kettle.
In some of the embodiments, a steam cooling detection sampling port is arranged in each distillation still.
In some embodiments, a stirring mechanism is arranged in each distillation kettle, and a program-controlled temperature rise heating device is arranged outside each distillation kettle.
The invention also aims to provide a method for continuously rectifying and recovering the solvent of the parallel solid-containing mother liquor.
A solvent continuous rectification recovery method of a parallel solid-containing mother liquor, a solvent continuous rectification recovery system using the parallel solid-containing mother liquor, comprises the following steps:
when a plurality of the distillation kettles are connected in parallel, the solution to be treated containing the solvent enters each distillation kettle to carry out kettle-type distillation, the distillation speed of at least one distillation kettle is controlled to be different from the distillation speeds of other distillation kettles, and the gas phase discharging of the other distillation kettles at the top of the kettle is realized when at least one distillation kettle contains solid material liquid discharging at the bottom of the kettle;
when the distillation kettle discharges in a solid phase manner at the bottom of the kettle, the liquid containing the solid material is pumped out by a discharge pump, and when the distillation kettle discharges in a gas phase manner, the produced steam is collected and then enters the rectifying tower;
the rectifying tower fractionates the vapor to form a light fraction and a heavy fraction.
In some embodiments, the controlling the distillation speed of at least one of the stills to be different from the distillation speeds of the other stills includes controlling the gas phase discharge speed of at least one of the stills to be higher than the gas phase discharge speeds of the other stills, controlling the feed speed of at least one of the stills to be lower than the feed speeds of the other stills, and controlling the distillation start time of at least one of the stills to be earlier than the distillation start time of the other stills.
In some embodiments, when the distillation start time of at least one of the stills is controlled to be earlier than the distillation start time of the other stills, the method specifically comprises the following steps:
controlling the distillation temperature T in the first distillation kettle, allowing the solution containing the solvent to be treated to enter the first distillation kettle for kettle distillation, and allowing the steam generated by the first distillation kettle to enter the rectifying tower;
after the first distillation kettle is distilled for a first preset time, the distillation temperature T in the second distillation kettle is controlled, the solution to be treated containing the solvent enters the second distillation kettle to be subjected to kettle distillation, and steam generated by the second distillation kettle enters the rectifying tower;
and analogizing in turn, after the distillation of the Nth-1 th preset time in the distillation kettle, controlling the distillation temperature T in the Nth distillation kettle, allowing the solution containing the solvent to be treated to enter the Nth distillation kettle for kettle distillation, allowing the steam produced by the Nth distillation kettle to enter the rectifying tower, and simultaneously controlling the first distillation kettle to stop gas-phase discharge and perform solid-containing liquid discharge at the bottom of the kettle.
The invention also aims to provide the application of the method for continuously rectifying and recovering the solvent of the parallel solid-containing mother liquor.
The application of the solvent continuous rectification recovery method of the parallel solid-containing mother liquor in the solvent recovery of the D-calcium pantothenate crystallization mother liquor is realized when a plurality of distillation kettles are connected in parallel: each of the stills was subjected to a distillation cycle of 12 hours per distillation, and the distillation temperature T was increased from 66 ℃ to 100 ℃ in each distillation cycle.
In conclusion, the parallel continuous solvent rectification and recovery system for the solid-containing mother liquor combines a plurality of batch rectifications into one continuous rectification, has large treatment capacity, is uninterrupted in rectification and improves rectification efficiency, and utilizes the vaporization heat of the general distilled solvent to directly enter a rectification tower without the processes of condensation and reboiling, thereby saving energy. A plurality of stills link sets up, realizes the dislocation distillation, guarantees rectifying column uninterrupted duty, and in the solid feed liquid ejection of compact that contains at the bottom of one or several stills, other stills can keep the ejection of compact of top gas phase, keep the air input that gets into the rectifying column and contain the component proportion invariable basically, and the quality of rectification is guaranteed in the setting of convenient rectification.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings used in the description of the embodiments will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the application, and that other drawings can be derived from these drawings by a person skilled in the art without inventive effort.
For a more complete understanding of the present application and its advantages, reference is now made to the following descriptions taken in conjunction with the accompanying drawings. Wherein like reference numerals refer to like parts in the following description.
FIG. 1 is a schematic view of a solvent continuous distillation recovery system of a parallel solid-containing mother liquor according to an embodiment of the present invention.
Description of the reference numerals
10. A parallel type solid-containing mother liquor solvent continuous rectification recovery system; 100. a distillation kettle; 200. a discharge pump; 300. a rectifying tower; 400. a reboiler; 500. a tower top condenser; 600. and (5) a product storage tank.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise.
In the present invention, unless otherwise explicitly stated or limited, the terms "mounted," "connected," "fixed," and the like are to be construed broadly, e.g., as being permanently connected, detachably connected, or integral; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be interconnected within two elements or in a relationship where two elements interact with each other unless otherwise specifically limited. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used herein are for illustrative purposes only and do not denote a unique embodiment.
In the description of the present invention, the meaning of a plurality is one or more, the meaning of a plurality is two or more, and the above, below, exceeding, etc. are understood as excluding the present numbers, and the above, below, within, etc. are understood as including the present numbers. If the first and second are described for the purpose of distinguishing technical features, they are not to be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated or implicitly indicating the precedence of the technical features indicated.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The embodiment of the application provides a parallel type continuous solvent rectification and recovery system 10 for solid-containing mother liquor, which is used for solving the problems that the traditional processing method is high in energy consumption and equipment investment, has multiple evaporation and condensation processes and is high in consumption of steam and circulating cooling water. The following description will be made with reference to the accompanying drawings.
Fig. 1 is a schematic structural view of a parallel type continuous solvent rectification and recovery system 10 for solid-containing mother liquor according to an embodiment of the present application. The parallel continuous solvent rectification and recovery system 10 for solid-containing mother liquor can be used for recovering the solvent containing the solid mother liquor.
In order to more clearly illustrate the structure of the system 10 for continuously rectifying and recovering the solvent of the parallel solid-containing mother liquor, the system 10 for continuously rectifying and recovering the solvent of the parallel solid-containing mother liquor will be described below with reference to the accompanying drawings.
Fig. 1 is a schematic structural diagram of a solvent continuous rectification recovery system 10 of parallel solid-containing mother liquor according to an embodiment of the present application. A parallel continuous solvent rectification and recovery system 10 for solid-containing mother liquor comprises a distillation assembly, a discharge pump 200, a rectifying tower 300, a reboiler 400 and an overhead condenser 500.
The distillation assembly includes a number of stills 100. A plurality of stills 100 are connected in parallel. A discharge pump 200 is connected to one or more stills 100 for solids-containing liquid discharge. The top of each still 100 is connected to a rectifying column 300 through a pipe. The top of each distillation still 100 is connected to the pipeline of the rectifying tower 300 and is provided with a control valve.
The rectifying tower 300 is used for collecting vapor of the distillation assembly and performing fractionation to form light fraction and heavy fraction.
A reboiler 400 is connected to the bottom of the rectification column 300 for reboiling the heavy fraction.
An overhead condenser 500 is connected to the top of the rectifying tower 300 for condensing the light fraction of the rectifying tower 300.
In some of these embodiments, the parallel solids mother liquor solvent continuous distillation recovery system 10 further comprises a product storage tank 600. Product tank 600 is connected to discharge pump 200 for collecting solids-containing liquid pumped by discharge pump 200.
In some of these embodiments, the number of stills 100 is 5 to 8. For example, in one particular example, the number of stills 100 is 5; in another specific example, the number of stills 100 is 8. Preferably, referring to fig. 1, the number of stills 100 is 6.
In some of these embodiments, still 100 has a volume of 2m 3 ～12m 3 . The volume of the distillation still 100 can be set according to actual needs.
In some of these embodiments, a level gauge is disposed within each still 100. The liquid level gauge is used to detect the liquid level in the distillation still 100.
In some embodiments, a steam cooling detection sampling port is disposed in each distillation still 100. The steam cooling detection sampling port is used for detecting the steam in the distillation still 100 after being cooled and sampled so as to match with each distillation still 100 for switching stage heating.
In some embodiments, each of the stills 100 is provided with a stirring mechanism therein. The stirring mechanism is used for stirring the liquid in the distillation kettle 100 to improve the evaporation speed.
In some embodiments, a programmed temperature-raising heating device is respectively arranged outside each distillation still 100. The program control heating device is used for accurately controlling the temperature of the temperature rise in different stages in the kettle, so that the steam components are more uniform.
The invention also aims to provide a method for continuously rectifying and recovering the solvent of the parallel solid-containing mother liquor.
A solvent continuous rectification recovery method of parallel solid-containing mother liquor, which uses a solvent continuous rectification recovery system 10 of the parallel solid-containing mother liquor, comprises the following steps:
when a plurality of distillation kettles 100 are connected in parallel, the solution to be treated containing the solvent enters each distillation kettle 100 for kettle-type distillation, the distillation speed of at least one distillation kettle 100 is controlled to be different from the distillation speed of other distillation kettles 100, and the solid-containing liquid of at least one distillation kettle 100 at the kettle bottom is discharged, and other distillation kettles 100 are discharged from the gas phase at the kettle top;
when the distillation kettle 100 discharges solid-containing liquid at the bottom of the kettle, the solid-containing liquid is pumped out by the discharge pump 200, and when the distillation kettle 100 discharges gas, the produced steam is converged and enters the rectifying tower 300;
the rectifying tower 300 fractionates the vapor to form a light fraction and a heavy fraction.
In some embodiments, the controlling the distillation speed of at least one distillation still 100 to be different from the distillation speeds of other distillation still 100 includes one or more of controlling the gas phase discharge speed of at least one distillation still 100 to be greater than the gas phase discharge speeds of other distillation still 100, controlling the feed speed of at least one distillation still 100 to be less than the feed speed of other distillation still 100, and controlling the distillation start time of at least one distillation still 100 to be earlier than the distillation start time of other distillation still 100.
In some embodiments, when the distillation start time of at least one distillation still 100 is controlled to be earlier than the distillation start time of other distillation still 100, the method specifically comprises the following steps:
controlling the distillation temperature T in the first distillation kettle 100, allowing the solution containing the solvent to be treated to enter the first distillation kettle 100 for kettle distillation, and allowing the steam generated by the first distillation kettle 100 to enter the rectifying tower 300;
after the first distillation kettle 100 is distilled for the first preset time, the distillation temperature T in the second distillation kettle 100 is controlled, the solution to be treated containing the solvent enters the second distillation kettle 100 for kettle distillation, and steam generated by the second distillation kettle 100 enters the rectifying tower 300;
and analogizing in turn, after the Nth-1 distillation kettle 100 distills the Nth-1 preset time, controlling the distillation temperature T in the Nth distillation kettle 100, allowing the solution containing the solvent to be treated to enter the Nth distillation kettle 100 for kettle distillation, allowing the steam produced by the Nth distillation kettle 100 to enter the rectifying tower 300, and simultaneously controlling the first distillation kettle 100 to stop gas-phase discharging and perform discharging of the solid material-containing liquid at the bottom of the kettle.
The invention also provides an application of the solvent continuous rectification recovery method of the parallel solid-containing mother liquor.
The application of the solvent continuous rectification recovery method of the parallel solid-containing mother liquor in the solvent recovery of the D-calcium pantothenate crystallization mother liquor is that when a plurality of distillation kettles 100 are connected in parallel:
each distillation still 100 was subjected to one distillation cycle per 12 hours of distillation, and the distillation temperature T was increased from 66 ℃ to 100 ℃ in each distillation cycle. Specifically, within 12 hours of distillation, six stages can be divided, the first stage, with time T1=0-2h, the distillation temperature T increasing gradually from 66 ℃ to 69 ℃; a second stage, time T2=2-4h, distillation temperature T is gradually increased from 69 ℃ to 73 ℃; a third stage, at a time T3=4-6h, in which the distillation temperature T is gradually increased from 73 ℃ to 79 ℃; a fourth phase, at a time T4=6-8h, with a distillation temperature T that is gradually increased from 79 ℃ to 88 ℃; a fifth stage, with time T5=8-10h, with distillation temperature T gradually increasing from 88 ℃ to 100 ℃; a sixth phase, time T6=10-12h, distillation temperature T maintained at 100 ℃.
The parallel type solid mother liquor-containing solvent continuous rectification recovery system 10 combines a plurality of batch rectifications into one continuous rectification, saves equipment, utilizes the vaporization heat of the general distilled solvent to directly enter the rectification tower 300, does not need the processes of condensation and reboiling, saves energy, is arranged in a linkage manner, keeps the mixed air inflow and the contained component proportion basically constant, is convenient for rectification arrangement, and ensures the rectification quality.
Example 1
This embodiment provides a parallel continuous solvent distillation recovery system 10 for solid-containing mother liquor.
A parallel continuous solvent rectification and recovery system 10 for solid-containing mother liquor comprises a distillation assembly, a discharge pump 200, a rectifying tower 300, a reboiler 400, an overhead condenser 500 and a product storage tank 600.
The distillation assembly comprises 6 distillation kettles 100, and the volume of the distillation kettle 100 is 5m 3 . The 6 stills 100 were connected in parallel. A liquid level meter is arranged in each distillation still 100. Each of the stills 100 is provided therein with a stirring mechanism.
The discharging pump 200 is connected with each distillation still 100 for discharging the solid-containing liquid. Product tank 600 is connected to discharge pump 200 for collecting solids-containing liquid pumped by discharge pump 200. The top of each still pot 100 is connected to a rectifying column 300. The top of each distillation still 100 is connected to a pipeline of the rectifying tower 300, and a control valve is provided on each pipeline.
The rectifying tower 300 is used for collecting vapor of the distillation assembly and performing fractionation to form light fraction and heavy fraction.
A reboiler 400 is connected to the bottom of the rectification column 300 for reboiling the heavy fraction.
The overhead condenser 500 is connected to the top of the rectifying tower 300 for condensing the light fraction discharged outside the rectifying tower 300.
Example 2
The embodiment provides a method for continuously rectifying and recovering a solvent of a parallel solid-containing mother solution.
A method for continuously rectifying and recovering a solvent of a parallel solid-containing mother liquor, which uses a system 10 for continuously rectifying and recovering the solvent of the parallel solid-containing mother liquor in example 1, comprises the following steps:
step 1, feeding the solution to be treated containing the solvent into each distillation kettle 100 for kettle-type distillation, wherein each distillation kettle 100 is used for distilling for 12 hours in a distillation cycle, and the distillation temperature T is increased from 66 ℃ to 100 ℃ in each distillation cycle. Within 12 hours of distillation, six stages can be divided, a first stage, time T1=0-2h, and distillation temperature T is gradually increased from 66 ℃ to 69 ℃; a second stage, time T2=2-4h, distillation temperature T is gradually increased from 69 ℃ to 73 ℃; a third stage, at a time T3=4-6h, in which the distillation temperature T is gradually increased from 73 ℃ to 79 ℃; a fourth stage, with time T4=6-8h, with distillation temperature T gradually increasing from 79 ℃ to 88 ℃; a fifth stage, with time T5=8-10h, with distillation temperature T gradually increasing from 88 ℃ to 100 ℃; in the sixth stage, time T6=10-12h, the distillation temperature T is maintained at 100 ℃.
Step 2, controlling the distillation starting time of one distillation kettle 100 to be earlier than the distillation starting time of other distillation kettles 100, so that the distillation speed of the distillation kettle 100 is different from the distillation speed of other distillation kettles 100, and realizing that when at least one distillation kettle 100 discharges solid phase at the bottom of the kettle, other distillation kettles 100 discharge gas phase at the top; the method specifically comprises the following steps:
controlling the distillation temperature T in the first distillation kettle 100, allowing the solution containing the solvent to be treated to enter the first distillation kettle 100 for kettle distillation, and allowing the steam generated by the first distillation kettle 100 to enter the rectifying tower 300;
after the first distillation kettle 100 is distilled for the first preset time, the distillation temperature T in the second distillation kettle 100 is controlled, the solution to be treated containing the solvent enters the second distillation kettle 100 for kettle distillation, and steam generated by the second distillation kettle 100 enters the rectifying tower 300;
by analogy, after the fifth distillation kettle 100 is distilled for the fifth preset time, the distillation temperature T in the sixth distillation kettle 100 is controlled, the solution to be treated containing the solvent enters the sixth distillation kettle 100 for kettle distillation, and the steam generated by the sixth distillation kettle 100 enters the rectifying tower 300. Meanwhile, the first distillation still 100 is controlled to stop gas-phase discharge and perform solid-phase discharge, and thus the amount and composition of the mixed steam entering the rectifying tower 300 are ensured to be substantially constant.
For example, the solvent initial concentration of the solution to be treated containing the solvent in the first distillation still 100 is 70%, the content of the vapor solvent distilled out in the first 2h (t 1) in the first distillation still 100 is 95% or more, and as time goes by, the content of the solvent in the solution to be treated containing the solvent in the first distillation still 100 gradually decreases, the content of the vapor solvent distilled out also gradually decreases; therefore, the content of the vapor solvent distilled in the second 2h (t 2) in the first distillation still 100 is 90%; the content of the vapor solvent distilled off in the third 2h (t 3) in the first distillation still 100 is 85%, the content of the vapor solvent distilled off in the fourth 2h (t 4) in the first distillation still 100 is 80%, the content of the vapor solvent distilled off in the fifth 2h (t 5) in the first distillation still 100 is 75%, and the content of the vapor solvent distilled off in the sixth 2h (t 6) in the first distillation still 100 is 50%.
The solvent-containing liquid to be treated in the second distillation still 100 was also set to have an initial concentration of the solvent of 70%. However, the second still 100 is opened only in the second 2h (t 2), that is, when the content of the vapor solvent distilled in the second 2h (t 3) of the first still 100 is 90%, the content of the vapor solvent distilled in the second 2h (t 2) of the second still 100 is 95%. The steam solvent content is between 90 and 95% after the distillate distilled from the first distillation still 100 and the distillate distilled from the second distillation still 100 are mixed in the steam pipeline.
Similarly, the solvent-containing liquid to be treated in the third distillation still 100 was set to have an initial concentration of 70%. The third distillation still 100 is opened only in the third 2h (t 3), when the content of the vapor solvent distilled by the first distillation still 100 in the third 2h (t 3) is 85%, and the content of the vapor solvent distilled by the second distillation still 100 in the third 2h (t 3) is 90%, the content of the vapor solvent distilled by the third distillation still 100 in the third 2h (t 3) is 95%, and the vapor of the first distillation still 100, the second distillation still 100 and the third distillation still 100 is mixed and then reaches a certain value between 85% and 95%.
By analogy, the fourth distillation still 100 is started in sequence, and the initial concentration of the solvent contained in the solution to be treated containing the solvent in the fourth distillation still 100 is also set to 70%. At the fourth 2h (t 5), the content of the vapor solvent distilled by the first distillation kettle 100 in the fourth 2h (t 4) is 80%; the fourth distillation still 100 distilled the vapor solvent content of 85% in the fourth 2h (t 4), the third distillation still 100 distilled the vapor solvent content of 90% in the fourth 2h (t 4), the fourth distillation still 100 distilled the vapor solvent content of 95% in the fourth 2h (t 4); the vapor mixing of the first to fourth stills 100 is a certain value between 80 to 95%.
The fifth distillation still 100 was sequentially started at the same time, and the initial concentration of the solvent contained in the solvent-containing liquid to be treated in the fifth distillation still 100 was also set to 70%. In the fifth 2h (t 5), the content of the vapor solvent distilled in the fifth 2h (t 5) of the first distillation kettle 100 is 75 percent; the content of the vapor solvent distilled in the fifth 2h (t 5) of the fourth distillation still 100 is 80%, the content of the vapor solvent distilled in the fifth 2h (t 5) of the third distillation still 100 is 85%, the content of the vapor solvent distilled in the fifth 2h (t 5) of the fourth distillation still 100 is 90%, and the content of the vapor solvent distilled in the fifth 2h (t 5) of the fifth distillation still 100 is 95%; the steam mixing of the five stills 100 is at a value between 75 and 95%.
And when the sixth 2h (t 6) begins, closing the first distillation kettle 100, opening the sixth distillation kettle 100 to start rectification, discharging the solid-containing liquid from the bottom of the first distillation kettle 100, and feeding the solid-containing liquid to the initial state for later use after the discharge is finished. The second still 100 is in the fifth 2h, the third still 100 is in the fourth 2h …, the sixth still 100 is in the first 2h, and the steam components of the five stills 100 are mixed to be a certain value between 75% and 95%.
When the seventh 2h begins, the second distillation kettle 100 is closed, the first distillation kettle 100 which was closed in the previous round is opened, the continuous gas phase discharge of the five distillation kettles 100 is still maintained, and the gas phase discharge components can still be kept constant after mixing.
And the like, and the process is continued.
And 3, when the distillation kettle 100 discharges the solid-containing liquid, pumping the solid-containing liquid to the product storage tank 600 by the discharge pump, and when the distillation kettle 100 discharges the gas phase, collecting the generated steam and then feeding the collected steam into the rectifying tower 300.
And 4, fractionating the steam by using the rectifying tower 300 to form a light fraction and a heavy fraction.
The mother liquor crystallized in the D-calcium pantothenate process is treated by adopting the parallel solid-containing mother liquor solvent continuous rectification recovery method of the embodiment, the mother liquor contains 5% of solids, 5% of water and 90% of methanol, parallel distillation is carried out by adopting the parallel solid-containing mother liquor solvent continuous rectification recovery method of the embodiment, combined steam enters rectification, and the data is as follows:
when the distillation device works, the feeding amount in each distillation kettle 100 is 10000Kg, each distillation is 12 hours, a cycle is formed, each distillation kettle 100 corresponds to the following six different stages respectively, and the gas-phase discharging steam component during discharging is relatively stable and fluctuates in a small range.
In the first stage, the time t1=0-2h, the evaporation steam accounts for 20% of the feeding amount, the average content of methanol in the steam is 96%, and the temperature of the distillation kettle 100 is gradually increased from 66 ℃ to 69 ℃.
In the second stage, the time t2=2-4h, the evaporation steam accounts for 20% of the feeding amount, the average content of methanol in the steam is 94%, and the temperature of the distillation kettle 100 is gradually increased from 69 ℃ to 73 ℃.
And in the third stage, the time t3=4-6h, the evaporation steam accounts for 20% of the feeding amount, the average content of the methanol in the steam is 92%, and the temperature of the distillation kettle 100 is gradually increased from 73 ℃ to 79 ℃.
And in the fourth stage, the time t4=6-8h, the evaporation steam accounts for 17% of the feeding amount, the average content of methanol in the steam is 90%, and the temperature of the distillation kettle 100 is gradually increased from 79 ℃ to 88 ℃.
In the fifth stage, the time t5=8-10h, the evaporation steam accounts for 15% of the feeding amount, the average content of methanol in the steam is 80%, and the temperature of the distillation kettle 100 is gradually increased from 88 ℃ to 100 ℃.
In the sixth stage, at time t6=10-12h, the evaporation residue was discharged in an amount of 8% of the feed amount.
In the above six stages, the combined steam amount is 10000Kg × (20% +20% +17% + 15%)/12h =9200kg/12h =766.6Kg/h, and the average methanol content in the combined steam is methanol: water =90:3.
detection shows that the speed of discharging light fraction of the rectifying tower is =740kg/h, and the content of methanol in the light fraction is more than 99.7%); the discharge speed of heavy fraction of the rectifying tower is =25.5kg/h, and the water content in the heavy fraction is more than 85%.
In summary, the parallel continuous solvent rectification and recovery system 10 for solid-containing mother liquor combines a plurality of batch rectifications into one continuous rectification, has large handling capacity, is uninterrupted in rectification, and improves rectification efficiency, and the parallel continuous solvent rectification and recovery system 10 for solid-containing mother liquor directly enters a rectification tower by using the vaporization heat of a general distilled solvent without the processes of condensation and reboiling, thereby saving energy. A plurality of stills 100 linkage sets up, realizes the dislocation distillation, guarantees rectifying column 300 uninterrupted duty, contains the solid feed liquid ejection of compact in the bottom of one or several stills 100 cauldron, and other stills 100 can keep the gaseous phase ejection of compact in top, keep the air input that gets into rectifying column 300 and contain the component proportion invariable basically, and the quality of rectification is guaranteed in the setting of convenient rectification.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to the related descriptions of other embodiments.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the present invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The utility model provides a solvent continuous rectification recovery system of solid mother liquor is contained to parallel, its characterized in that, includes distillation subassembly, rectifying column, reboiler and top of the tower condenser, the distillation subassembly includes a plurality of stills, and is a plurality of stills parallel connection, it is a plurality of the discharging pipe is connected alone or jointly at the bottom of stills's the cauldron, each still's top all through the pipe connection in the rectifying column, each still's top connect in be provided with control flap on the pipeline of rectifying column respectively, the rectifying column is used for collecting the steam of distillation subassembly and fractionate and form light fraction and heavy fraction, the reboiler connect in the bottom of rectifying column is in order to be used for reboiling to heavy fraction, the top of the tower condenser connect in the top of rectifying column is in order to be used for right the rectifying column light fraction condenses.
2. The system for continuously rectifying and recovering the solvent of the parallel solid-containing mother liquor according to claim 1, further comprising a discharge pump and a product storage tank, wherein the discharge pump is connected with the discharge pipe, and the product storage tank is connected with the discharge pump to collect the concentrated solid-containing liquid at the bottom of the distillation kettle.
3. A parallel solid-containing mother liquor solvent continuous rectification recovery system according to claim 1 is characterized in that the number of the distillation kettles is 5-8.
4. A system for the continuous rectification and recovery of solvents in parallel solid-containing mother liquor according to any one of claims 1 to 3, characterized in that the volume of the distillation kettle is 2m 3 ～12m 3 。
5. A parallel solid-containing mother liquor solvent continuous rectification recovery system according to any one of claims 1 to 3, characterized in that a liquid level meter and/or a steam cooling detection sampling port is arranged in each distillation kettle.
6. A parallel solid-containing mother liquor solvent continuous rectification recovery system according to any one of claims 1 to 3 characterized in that each distillation still is provided with a stirring mechanism and a program controlled temperature rise heating device.
7. A method for continuously rectifying and recovering a solvent of a parallel solid-containing mother liquor is characterized in that the system for continuously rectifying and recovering the solvent of the parallel solid-containing mother liquor, which is disclosed by any one of claims 1 to 6, is used, and comprises the following steps:
when a plurality of the distillation kettles are connected in parallel, the solution to be treated containing the solvent enters each distillation kettle to carry out kettle-type distillation, the distillation speed of at least one distillation kettle is controlled to be different from the distillation speeds of other distillation kettles, and the gas phase discharging of the other distillation kettles at the top of the kettle is realized when at least one distillation kettle contains solid material liquid discharging at the bottom of the kettle;
when the distillation kettle discharges at the bottom of the kettle, solid-containing material liquid is pumped out by a discharging pump, and when the distillation kettle discharges in a gas phase, generated steam is collected and enters the rectifying tower;
the rectifying tower fractionates the vapor to form a light fraction and a heavy fraction.
8. A solvent continuous rectification recovery method of a parallel solid-containing mother liquor according to claim 7, characterized in that when the distillation speed of at least one of the stills is controlled to be different from the distillation speeds of the other stills, the method comprises one or more of controlling the gas phase discharge speed of at least one of the stills to be higher than the gas phase discharge speeds of the other stills, controlling the feed speed of at least one of the stills to be lower than the feed speeds of the other stills, and controlling the distillation start time of at least one of the stills to be earlier than the distillation start time of the other stills.
9. A parallel type continuous solvent distillation and recovery method for solid-containing mother liquor according to claim 7, wherein when the distillation start time of at least one distillation still is controlled to be earlier than the distillation start time of other distillation still, the method specifically comprises the following steps:
controlling the distillation temperature T in the first distillation kettle, allowing the solution to be treated containing the solvent to enter the first distillation kettle for kettle distillation, and allowing the steam generated by the first distillation kettle to enter the rectifying tower;
after the first distillation kettle is distilled for a first preset time, the distillation temperature T in the second distillation kettle is controlled, the solution to be treated containing the solvent enters the second distillation kettle to be subjected to kettle distillation, and steam generated by the second distillation kettle enters the rectifying tower;
and analogizing in sequence, after the distillation kettle distills for the Nth-1 preset time, controlling the distillation temperature T in the distillation kettle for the Nth, allowing the solution to be treated containing the solvent to enter the Nth distillation kettle for kettle-type distillation, allowing the steam produced by the distillation kettle for the Nth distillation to enter the rectifying tower, and simultaneously controlling the first distillation kettle to stop gas-phase discharging and perform discharging of the solution containing solid materials at the bottom of the kettle.
10. Use of a process for the continuous solvent distillation recovery of a parallel solids-containing mother liquor according to any one of claims 7 to 9 for the recovery of solvent from a D-calcium pantothenate crystallization mother liquor, characterized in that, when a plurality of said stills are connected in parallel:
each of the stills was subjected to a distillation cycle of 12 hours per distillation, and the distillation temperature T was increased from 66 ℃ to 100 ℃ in each distillation cycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211040643.XA CN115317942A (en) | 2022-08-29 | 2022-08-29 | Parallel type solid-containing mother liquor solvent continuous rectification recovery system and method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211040643.XA CN115317942A (en) | 2022-08-29 | 2022-08-29 | Parallel type solid-containing mother liquor solvent continuous rectification recovery system and method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115317942A true CN115317942A (en) | 2022-11-11 |
Family
ID=83928346
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211040643.XA Pending CN115317942A (en) | 2022-08-29 | 2022-08-29 | Parallel type solid-containing mother liquor solvent continuous rectification recovery system and method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115317942A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT509173A1 (en) * | 2009-12-02 | 2011-06-15 | Schauer Rudolf Ing Dipl Ing Fh | BIODIESEL PRODUCTION PLANT |
| CN202844611U (en) * | 2012-10-08 | 2013-04-03 | 江苏省格林艾普化工股份有限公司 | Distillation device system for recovering chloroactic acid mother liquor |
| CN107011122A (en) * | 2017-05-16 | 2017-08-04 | 扬州联博药业有限公司 | A kind of method for reclaiming the ethanol in medical industry mother liquor |
-
2022
- 2022-08-29 CN CN202211040643.XA patent/CN115317942A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT509173A1 (en) * | 2009-12-02 | 2011-06-15 | Schauer Rudolf Ing Dipl Ing Fh | BIODIESEL PRODUCTION PLANT |
| CN202844611U (en) * | 2012-10-08 | 2013-04-03 | 江苏省格林艾普化工股份有限公司 | Distillation device system for recovering chloroactic acid mother liquor |
| CN107011122A (en) * | 2017-05-16 | 2017-08-04 | 扬州联博药业有限公司 | A kind of method for reclaiming the ethanol in medical industry mother liquor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7572353B1 (en) | Ethanol distillation process | |
| CN100586523C (en) | Pleietrepie counter current falling film evaporator for recycling organic solvent | |
| CN105836951B (en) | A kind of electroplating waste processing process and device | |
| US4327184A (en) | Inert-gas stripping and distillation apparatus | |
| CN104973638B (en) | Processing technology of high-salt high-concentration organic waste liquid | |
| CN102482213B (en) | NMP distilling apparatus | |
| CN104178406B (en) | A kind of energy-efficient white wine continuous distillation method and device thereof | |
| WO2020155571A1 (en) | Separation and recycle system for water-containing organic waste liquid and organic solvent, and recycle method | |
| CN206553207U (en) | It is a kind of to be used for the apparatus system of cobaltous sulfate efficient concentration and continuous crystallisation | |
| CN107188199A (en) | It is a kind of that ammonium sulfate, the Processes and apparatus of sodium sulphate are reclaimed from waste water | |
| CN204502433U (en) | Flash distillation scraper concentrator | |
| CN105327518A (en) | Pentanediamine concentration system and method thereof | |
| CN110183325A (en) | A kind of the purification recovery process and device of acetic acid waste liquid | |
| CN211445385U (en) | Contain organic solvent's salt waste water evaporation equipment | |
| US3527676A (en) | Multistage distillation for desalinizing saline water | |
| CN111514602B (en) | Method and device for removing dichloromethane in high-boiling-point thermosensitive material | |
| CN109320417A (en) | Utilize the device and method of partition tower purification Ergol | |
| CN115317942A (en) | Parallel type solid-containing mother liquor solvent continuous rectification recovery system and method and application thereof | |
| CN108467351A (en) | A kind of adiponitrile refining system | |
| US1822454A (en) | Process and apparatus for the simultaneous distillation | |
| CN100425587C (en) | Method for azeotropic distillation | |
| CN207012590U (en) | A kind of dehydration of organic solvent system | |
| CN105884106A (en) | Benzene hydrogenation wastewater desulfurization and deamination treatment method aiming at improving deamination and treatment device applying same | |
| CN218357428U (en) | Serial-type rectification recovery device | |
| CN216777931U (en) | Vacuum purification device of methyl pyrrolidone waste liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |